Hydrochloric Acid → HCID 136337782, compound

Participants

Reaction Steps

The product from Example 26.6 (0.055 g, 0.16 mmol) was stirred in a 1% hydrogen chloride solution in methanol (10 ml) for 1.5 h at ambient temperature. The reaction mixture was neutralised with Amberlyst A-21 ion exchange resin. The resin was filtered and the reaction solution concentrated. The residue was chromatographed (methanol [3.5N ammonia solution]-DCM, 1:4) giving a white solid (0.035 g, 72%). 1H NMR (CD3OD) δ ppm 7.98 (s, 1H), 7.60 (s, 1H), 4.44 (ABq, 2H), 3.97 (q, J=3.8 Hz, 1H), 3.76 (dd, J=11.7, 4.2 Hz, 1H), 3.67 (dd, J=11.7, 3.8 Hz, 1H), 3.44 (m, 1H), 2.92 (m, 2H), 2.08 (s, 3H). 13C NMR (CD3OD) δ 156.2, 145.6, 144.0, 130.7, 120.0, 109.8, 70.1, 66.0, 60.0, 41.4, 33.9, 16.0. +ESMS Found 299.1194: (M+H)+ C12H19N4O3S requires 299.1178:

Provenance & Evidence